CN108220486A - A kind of method for detaching saccharic acid using sour Retarding resin - Google Patents
A kind of method for detaching saccharic acid using sour Retarding resin Download PDFInfo
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- CN108220486A CN108220486A CN201711463700.4A CN201711463700A CN108220486A CN 108220486 A CN108220486 A CN 108220486A CN 201711463700 A CN201711463700 A CN 201711463700A CN 108220486 A CN108220486 A CN 108220486A
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- Prior art keywords
- acid
- resin
- saccharic acid
- sour
- method described
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Classifications
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K1/00—Glucose; Glucose-containing syrups
- C13K1/02—Glucose; Glucose-containing syrups obtained by saccharification of cellulosic materials
- C13K1/04—Purifying
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Saccharide Compounds (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a kind of methods for detaching saccharic acid using sour Retarding resin, saccharic acid mixed liquor is handled through sour means of retardation, equipped with a kind of using Chioro-anion exchange resin as the sour Retarding resin of stationary phase in sour means of retardation, acid in separation process in saccharic acid mixed liquor is arrested in resin, and glucide is directed through resin and flows out in advance, regeneration that is de-, and completing resin is washed with deionized water after the completion of sample introduction.The present invention can separate the saccharic acid in saccharic acid mixed liquor, and the saccharic acid rate of recovery is high, and the regeneration of resin is achieved that with deionized water.
Description
Technical field
The present invention relates to renewable new energy source technical field, more particularly to a kind of side that saccharic acid is detached using sour Retarding resin
Method.
Background technology
There is an urgent need to produce the regenerative resources such as alcohol fuel by raw material of lignocellulosic for environmental pollution and energy crisis.
The key of cellulosic ethanol is that cellulosic raw material is converted into the utilizable monosaccharide of microorganism, and acid catalyst can effective water
Solve lignocellulosic generation monosaccharide.Iranmahboob etc. with 26% sulphuric acid hydrolysis sawdust sugar yield up to more than 78%,
Heinonen etc. reports concentrated acid method hydrocellulose and possesses 80% even higher sugared yield, but how efficient, low cost point
It is then very difficult from carbohydrate and acid catalyst.
There is sugar/acid separation main method in hydrolyzate of the cellulose after acid catalysis：Neutralisation, solvent extraction, electric osmose
Analysis method and chromatography.Neutralisation is that a kind of industrial saccharic acid separation method more often applied, neutralizer are generally made a living at present
Lime, the slightly solubility calcium sulfate of generation can be removed by precipitating the method for filtering, but since catalysis acid can not recycle and
It causes greatly to waste.In addition, some researches show that the total reducing sugar loss up to 10% using neutralisation, further increase and be produced into
This.Electroosmose process will not lead to the loss of sugar, but it consumes a large amount of electric energy, and equipment manufacturing cost is expensive, operating cost
It is high.Solvent extraction is to achieve the purpose that sour sugar from although should by the way that inorganic acid extraction is entered appropriate organic solvent
Low energy consumption for method, but due to there are the dissolving of solvent, emulsion, micro solvent being usually contained in raffinate phase, to rear supervention
Ferment process has an adverse effect, it usually needs is further processed.Patent No. 201010101585.8《A kind of glycosylated degradation
The technique that spirit distiller grain prepares fermentable sugars》One kind is disclosed to be saccharified by the drying of Bai Jiu Lost grains, crushing, degradation and handed over using ion
It changes resin and carries out the process that saccharic acid separation prepares fermentable sugars, this is simple for process, operation is easy, but the saccharic acid rate of recovery is low, has two
Secondary pollution.
Ion retardation method is initially in 1963, by Hatch and Dillon report separating acids and its corresponding acid salt
Process is alternatively referred to as acid retardance when it is applied to separating acid and non-acid blend.For the sour Retarding resin of acid retardance separation
There is the affinity of bigger to acid, it blocks acid in resin, and its acid salt is eluted away first, and then acid also elutes
Going out resin, this process follows two balances, and one is Donnan balances, the other is electric quantity balancing, when the two balances
When being broken, mixed solution, which is also separated, to be come.
The present invention proposes a kind of method for detaching saccharic acid using sour Retarding resin, which is that a kind of price is relatively low
Honest and clean, simple for process process, can realize saccharic acid is separated and recovered from catalyst inorganic acid, and resin eluent is only pure
Water does not consume other chemical reagent.
Invention content
The purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art, provides a kind of sour Retarding resin of utilization and detach
The method of saccharic acid.
To achieve these goals, the technical solution adopted in the present invention includes the following steps：
1) saccharic acid detaches：Saccharic acid mixed liquor is handled through sour means of retardation, in separation process in saccharic acid mixed liquor
Acid is arrested in resin, and glucide is directed through resin and flows out in advance, is washed with deionized water after the completion of sample introduction de-；
2) resin regeneration：Sour Retarding resin is carried out with deionized water to be eluted to balance.
Further, the saccharic acid mixed liquor described in step 1) can be saccharic acid mixed solution, and sugar therein can be grape
The glucides such as sugar, xylose, arabinose it is one or more, here for convenience by taking glucose as an example, mass concentration exists
2%-20%；Acid therein can be sulfuric acid, hydrochloric acid or nitric acid etc., here by taking sulfuric acid or hydrochloric acid as an example, the wherein quality of sulfuric acid
A concentration of 1%-30%, the mass concentration of hydrochloric acid is 1%-10%.
Further, the saccharic acid mixed liquor described in step 1) can also be lignocellulosic acid hydrolysis liquid, in acid retardance point
It need to be filtered to remove solid residue from before processing.The acquisition of lignocellulosic acid hydrolysis liquid in the present invention：First, using first
The lignocellulosic materials such as sour and a small amount of hydrochloric acid pretreated straw, corncob are to remove wherein most hemicelluloses and wooden
Element, residual solid (main component is cellulose) obtained by separation of solid and liquid hydrolyze after washing is dried through two step sulfuric acid process, Ran Houjing
The lignocellulosic acid hydrolysis liquid that centrifugal filtration obtains.
Further, the optimum condition of sour retardance process is point that sour Retarding resin is filled in sour means of retardation in step 1)
It is 1 from column diameter and the ratio of packed height:15-1:25, feed temperature is 45-55 DEG C, air speed 1.0-2.0h-1。
Further, the condition that sour Retarding resin is eluted to balance in step 2) is that the pH value of eluent is 7 or so.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, sour retardance process can efficiently separate the sugar and acid in saccharic acid mixed liquor, and the rate of recovery of saccharic acid be also maintained at compared with
High level.
2nd, the de- regeneration for achieving that sour Retarding resin is only washed with deionized water, it is simple and convenient, without other chemical reagent,
Alleviate environmental pressure.
3rd, during lignocellulosic acid hydrolysis liquid saccharic acid detaches, it is found that the process can not only efficiently separate sugar
Acid, and fermentation inhibitor is practically free of in the sugared eluent of gained, illustrate that the process has the effect of removing fermentation inhibitor simultaneously
Fruit simplifies technological process.
Specific embodiment
The present invention is described further with reference to specific implementation case.It describes in one embodiment of the invention
Elements and features can be combined with the elements and features shown in one or more other embodiments.It should be noted that
For purposes of clarity, component unrelated to the invention, known to persons of ordinary skill in the art or processing are omitted in explanation
Expression and description.
Example 1
Using the mixed solution of the hydrochloric acid (1%-10%) of different content and glucose (2%-20%) as raw material, with 1.0-
2.0h-1Air speed enter equipped with sour Retarding resinThe splitter of A-32Fine mesh, separation column diameter and filling
The ratio of height is 1:15-1:25, operation temperature is 45-55 DEG C, and adding in deionized water after the completion of sample introduction with identical flow velocity carries out
It elutes, the rate of recovery of hydrochloric acid is up to 90.4-96.9% in whole process, and the rate of recovery of glucose is up to 92.7%-99.1%.
Example 2
Using the mixed solution of the sulfuric acid (1%-30%) of different content and glucose (2%-20%) as raw material, with 1.0-
2.0h-1Air speed enter equipped with sour Retarding resinThe splitter of A-32Fine mesh, separation column diameter and filling
The ratio of height is 1:15-1:25, operation temperature is 45-55 DEG C, and adding in deionized water after the completion of sample introduction with identical flow velocity carries out
It elutes, the rate of recovery of sulfuric acid is up to 91.2-98.9% in whole process, and the rate of recovery of glucose is up to 93.8%-99.2%.
Example 3
The maize straw acid hydrolysis liquid of gained is after centrifugal filtration is handled, with 1.0h-1Air speed enter equipped with acid retardance set
FatThe splitter of A-32Fine mesh, the ratio for detaching column diameter and packed height is 1:25, operation temperature is
50 DEG C, sample introduction adds in deionized water with identical flow velocity after the completion and is eluted, and the condition that sugared eluent stops collecting is pH<2.3
The condition that sour eluent stops collecting is pH<3.2, with realize under the premise of saccharic acid separates as much as possible recycling sugar and
Acid, and meet culture solution pH needed for subsequent ethanol fermentation.The sugared eluent and sulfur acid of the 21.0g/L containing glucose can finally be obtained
5.0% sour eluent, wherein the glucose rate of recovery is up to 99.1%, and retrieval of sulfuric acid rate is up to 98.9%.Experimental study is also
It was found that the process can effectively remove the fermentation inhibitor in hydrolyzate, stalk acid hydrolysis liquid mainly forms comparison and sees before and after process
Table 1.
1 acid retardance of table hydrolyzate composition variation before and after the processing
Although the present invention and its advantage is described in detail it should be appreciated that without departing from by appended claim
Various changes, replacement and transformation can be carried out in the case of the spirit and scope of the present invention limited.Moreover, the model of the application
Enclose the specific embodiment for being not limited only to the described process of specification, method and steps.One of ordinary skilled in the art from
The disclosure performs and the corresponding basic phase of embodiment described herein it will be readily understood that can be used according to the present invention
Same function either obtains result, existing and in the future to be developed process, method or the step essentially identical with it.Cause
This, appended claim is intended to include such process, method or step in the range of them.
Claims (7)
- A kind of 1. method for detaching saccharic acid using sour Retarding resin, it is characterised in that：Saccharic acid mixed liquor is handed over through chlorine type anion Resin treatment is changed, the acid in separation process in feed liquid is arrested in resin, and glucide is directed through resin and flows out in advance.
- 2. according to the method described in claim 1, it is characterized in that：The ratio of sour Retarding resin separation column diameter and packed height It is 1:15-1:25, feed temperature is 45-55 DEG C, air speed 1.0-2.0h-1。
- 3. according to the method described in claim 1, it is characterized in that：The Chioro-anion exchange resin is A- 32 Fine mesh resins.
- 4. according to the method described in claim 1, it is characterized in that：The saccharic acid mixed liquor sugar therein is glucose, wood One or more mixtures of sugar, arabinose.
- 5. according to the method described in claim 1, it is characterized in that：The acid is one kind or more of sulfuric acid, hydrochloric acid or nitric acid Kind mixture.
- 6. according to the method described in claim 1, it is characterized in that：The saccharic acid mixed liquor is lignocellulosic sour water solution Liquid.
- 7. according to the method described in claim 1, it is characterized in that：Chioro-anion exchange resin eluted by deionized water, Regeneration.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711463700.4A CN108220486A (en) | 2017-12-28 | 2017-12-28 | A kind of method for detaching saccharic acid using sour Retarding resin |
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|---|---|---|---|
| CN201711463700.4A CN108220486A (en) | 2017-12-28 | 2017-12-28 | A kind of method for detaching saccharic acid using sour Retarding resin |
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| CN108220486A true CN108220486A (en) | 2018-06-29 |
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Citations (7)
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|---|---|---|---|---|
| CN1270538A (en) * | 1997-08-04 | 2000-10-18 | 受控的环境系统有限公司 | Method for separation of acid from sugars |
| JP4064359B2 (en) * | 2004-02-27 | 2008-03-19 | 純一 根本 | Method for separating phosphoric acid and lignocellulose hydrolysis product and method for producing glucose |
| CN101516821A (en) * | 2006-08-18 | 2009-08-26 | 艾欧基能源公司 | Process for obtaining an organic salt or organic acid from an aqueous sugar stream |
| WO2011097468A2 (en) * | 2010-02-05 | 2011-08-11 | Calera Corporation | Acid separation by acid retardation on an ion exchange resin in an electrochemical system |
| CN102282264A (en) * | 2009-01-14 | 2011-12-14 | 艾欧基能源公司 | Improved method for the production of glucose from lignocellulosic feedstocks |
| CN102600640A (en) * | 2012-01-09 | 2012-07-25 | 中德瑞生物炼制实验室(厦门)有限公司 | Method for separating sugar, acid and salt of lignocellulose hydrolysate |
| CN104611391A (en) * | 2013-11-05 | 2015-05-13 | 中国石油化工股份有限公司 | Method for preparing hydrolysis sugar from lignocellulose raw material |
-
2017
- 2017-12-28 CN CN201711463700.4A patent/CN108220486A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1270538A (en) * | 1997-08-04 | 2000-10-18 | 受控的环境系统有限公司 | Method for separation of acid from sugars |
| JP4064359B2 (en) * | 2004-02-27 | 2008-03-19 | 純一 根本 | Method for separating phosphoric acid and lignocellulose hydrolysis product and method for producing glucose |
| CN101516821A (en) * | 2006-08-18 | 2009-08-26 | 艾欧基能源公司 | Process for obtaining an organic salt or organic acid from an aqueous sugar stream |
| CN102282264A (en) * | 2009-01-14 | 2011-12-14 | 艾欧基能源公司 | Improved method for the production of glucose from lignocellulosic feedstocks |
| WO2011097468A2 (en) * | 2010-02-05 | 2011-08-11 | Calera Corporation | Acid separation by acid retardation on an ion exchange resin in an electrochemical system |
| CN102600640A (en) * | 2012-01-09 | 2012-07-25 | 中德瑞生物炼制实验室(厦门)有限公司 | Method for separating sugar, acid and salt of lignocellulose hydrolysate |
| CN104611391A (en) * | 2013-11-05 | 2015-05-13 | 中国石油化工股份有限公司 | Method for preparing hydrolysis sugar from lignocellulose raw material |
Non-Patent Citations (3)
| Title |
|---|
| JIANJUN LIU: "Separation of the acid-sugar mixtures by using acid retardation and further concentration of the eluents by using continuous-effect membrane distillation", 《J CHEM TECHNOL BIOTECHNOL》 * |
| 刘建军: "以秸秆为原料生产生物丁醇过程中关键问题的研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
| 刘跃红: "酸阻滞法用于白酒丢糟浓硫酸降解液糖酸分离的研究", 《食品工业》 * |
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Application publication date: 20180629 |